CN104697827A - Preparation and thermal analysis method of alloy sample containing high-volatility elements with high reaction activity - Google Patents
Preparation and thermal analysis method of alloy sample containing high-volatility elements with high reaction activity Download PDFInfo
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- CN104697827A CN104697827A CN201410670337.3A CN201410670337A CN104697827A CN 104697827 A CN104697827 A CN 104697827A CN 201410670337 A CN201410670337 A CN 201410670337A CN 104697827 A CN104697827 A CN 104697827A
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Abstract
The invention discloses a preparation and thermal analysis method of an alloy sample containing high-volatility elements with high reaction activity. The preparation and thermal analysis method comprises the following steps: (1) weighing alloy powder containing high-volatility elements with high reaction activity in a glove box, mixing uniformly and pressing for forming; (2) sealing a formed sample into a tantalum pipe, taking the tantalum pipe out of the glove box, sealing the tantalum pipe into a vacuum quartz tube, and then performing sintering and annealing treatment in a heat treatment furnace; and (3) taking the quartz tube out of the heat treatment furnace, quenching rapidly and taking the tantalum pipe out, and taking out the sample from the tantalum pipe in the glove box. The method can be widely applied to preparation and thermal analysis of the alloys containing high-volatility elements with high reaction activity, such as magnesium alloy containing aluminum, zinc and the like, rare earth alloy containing manganese, strontium, yttrium, neodymium and the like. The result of comparison with the melting point of the standard pure metal substance shows that the phase transition temperature precision determined by the thermal analysis method can reach +/-1 DEG C.
Description
Technical field
The present invention relates to a kind of containing high volatile volatile, the sample preparation of high reaction activity mischmetal and heat analysis method.
Background technology
The alloys such as magnesium, aluminium, zinc, as the structural metallic materials of loss of weight, have specific strength and specific stiffness is high, heat-conductivity conducting performance is good, be easy to processing and the easy feature such as recovery, are widely used in fields such as communications and transportation, electronic communication, Aero-Space.Thermal analyses can provide the phase transition temperature of material, to research material solidify and the material preparation process such as solid-state phase changes has great importance.The low boiling of the elements such as magnesium, aluminium, zinc brings great challenge to investigation and application.At present, traditional method is prepared alloy and is needed tens grams even the pure element raw material of several kilograms.Open method of smelting greatly wastes raw metal, and the metallic vapour of volatilization pollutes the environment, and part metals steam also has severe toxicity.In addition, open melting often can cause liquid metal to splash, and causes security incident.Not containing the material of high volatile volatile, high reaction activity element, its thermal analyses in non-protected atmosphere, prepares sample and carries out in the crucible opened wide.Magnesium alloy for containing high volatilization, high reaction activity element: on the one hand due to the high reaction activity of element, the sample prepared in non-protected atmosphere easily and water, oxygen react; On the other hand due to the high volatile volatile of magnesium, along with the rising of temperature in thermal analyses process, the vapour pressure of metal continues to raise.In open crucible, the metallic vapour volatilized constantly is discharged, thus result in the serious volatilization of sample, and damages thermal analyzer.These two factor actings in conjunction, cause conventional heat analysis method can not be used for the mensuration of the phase transition temperature of the alloy such as magnesium, aluminium, zinc containing high volatilization, high reaction activity element, thus cause alloy phase diagram, the phase change data such as existing magnesium, aluminium, zinc very rare.
Summary of the invention
The object of this invention is to provide a kind of containing high volatile volatile, the preparation of high reaction activity mischmetal and heat analysis method.
In order to achieve the above object, of the present invention containing high volatile volatile, high reaction activity mischmetal sample preparation methods, comprise the following steps:
(1) in glove box, take the alloy powder containing high volatile volatile, high reaction activity element, to mix and compressing;
(2) shaping specimen enclosure is entered in tantalum pipe, then tantalum pipe is taken out from glove box, enclose in vitreosil pipe, put into heat-treatment furnace subsequently and carry out sintering and annealing in process;
(3) quartz ampoule taken out rapid quench from heat-treatment furnace and tantalum pipe is taken out, then in glove box, sample being taken out from tantalum pipe.
Preferably, described alloy powder is magnesium alloy powder or Al alloy powder or Zinc alloy powder or manganese alloy powder or strontium alloy powder or yittrium alloy powder or neodymium alloy powder, and wherein the content of high volatile volatile, high reaction activity element magnesium, aluminium, zinc, manganese, strontium, yttrium, neodymium is respectively 99.0wt% ~ 99.99wt%.
As improvement, in alloy sample preparation process, sample water oxygen content is kept to be 0.4 ~ 1.0ppm.
Heat analysis method containing high volatile volatile, high reaction activity mischmetal sample of the present invention, comprises the following steps:
(1) in glove box, take the alloy powder containing high volatile volatile, high reaction activity element, to mix and compressing;
(2) shaping specimen enclosure is entered in tantalum pipe, then tantalum pipe is taken out from glove box, enclose in vitreosil pipe, put into heat-treatment furnace subsequently and carry out sintering and annealing in process;
(3) quartz ampoule taken out rapid quench from heat-treatment furnace and tantalum pipe is taken out, then in glove box, sample being taken out from tantalum pipe;
(4) sample of sample as differential scanning calorimetric analysis of one piece of heavy 25 ~ 60mg is cut, tantalum lid is suppressed with tantalum piece, by one end of intubating length about 10 ~ 20mm tantalum pipe bottom tantalum lid, and keep the bottom margin of the top of tantalum lid and tantalum pipe to flush, then by tantalum lid and tantalum pipe welded seal in glove box;
(5) in glove box, the sample of well cutting put into tantalum pipe and sealed, the tantalum pipe being sealed with sample is enclosed in vitreosil pipe outward at glove box, then quartz ampoule is put into heat-treatment furnace to anneal, after completing, tantalum pipe is taken out, insert differential scanning calorimetric analysis instrument support and carry out differential thermal analysis (DTA).
Preferably, described alloy powder is magnesium alloy powder or Al alloy powder or Zinc alloy powder or manganese alloy powder or strontium alloy powder or yittrium alloy powder or neodymium alloy powder, and wherein the content of high volatile volatile, high reaction activity element magnesium, aluminium, zinc, manganese, strontium, yttrium, neodymium is respectively 99.0wt% ~ 99.99wt%.
As improvement, in the thermal analyses process of alloy sample, sample water oxygen content is kept to be 0.4 ~ 1.0ppm.
The negative effect that contained by the alloys such as gordian technique to be solved by this invention is magnesium, aluminium, zinc, high volatile volatile and high reaction activity bring sample preparation and thermal analyses.For the high reaction activity of the alloys such as magnesium, aluminium, zinc, a low-moisture environment of hypoxemia must be formed, ensure that sample does not react with oxygen and water.The present invention adopts glove box to ensure that the alloys such as magnesium, aluminium, zinc keep lower water oxygen content to thermal analyses overall process from preparation.Glove box is filled with in casing by high purity inert gas (argon gas, nitrogen etc.), and be circulated throughout the experimental facilities of the active substance filtered wherein.In glove box, first the content of water and oxygen is reduced to below 1ppm, starts the preparation and determination methods of alloy sample subsequently.This ensures that thering alloy sample can not with oxygen and water reaction.For the high volatile volatile of the alloys such as magnesium, aluminium, zinc, the present invention devises the tantalum crucible of sealing.By in glove box, alloy sample sealing is loaded in tantalum crucible, make the metallic vapour volatilized rest on tantalum crucible inside, and then ensure that the mass loss of sample is less.Prepare an alloy sample and only need about 0.4 ~ 0.6 gram of raw metal, classic method is prepared an alloy and is needed a few hectogram even several kilograms of raw metals.The sample that the invention solves containing high volatile volatile, high reaction activity element is difficult to preparation and a thermoanalytical difficult problem.The method provided can be widely used in preparation and the thermal analyses thereof that magnesium (aluminium, zinc etc.) alloy, rare earth (manganese, strontium, yttrium, neodymium etc.) alloy etc. contain the alloy of high activity and high volatile volatile element.The fusing point contrast being belonged to material by same sterling gold shows that the phase transition temperature precision adopting heat analysis method of the present invention to measure can reach ± 1 ° of C.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
(1) in glove box, adopt magnesium granules (99.9 wt.%), zinc particle (99.9 wt.%), aluminium powder (99.9 wt.%), Argent grain (99.9 wt.%), take 50mg respectively with electronic balance;
(2) sample weighed up is sealed in tantalum pipe (external diameter 6.8mm, wall thickness 0.4mm, length 15mm), the tantalum crucible being sealed with sample is taken out from glove box, bottom is polished flat;
(3) support of the tantalum crucible of good seal being inserted differential scanning calorimetric analysis instrument carries out thermal analyses.
The fusing point contrast being belonged to material by same sterling gold shows that the phase transition temperature precision adopting heat analysis method of the present invention to measure can reach ± 1 ° of C.
Embodiment 2:
For sample preparation and the thermal analyses of binary system Mg-Sr, specific implementation process is as follows:
(1) in glove box, magnesium powder (99.5 wt.%) is adopted, strontium block (99.5 wt.%), 3 samples that weight is about 500mg are taken with electronic balance, after mixing, adopting small-sized electric sheeter to be pressed into diameter 5mm, is highly the cylinder of 6mm;
(2) with argon-arc welder, small column being encapsulated into external diameter is 7mm, wall thickness 0.3mm, and length is in the tantalum pipe of 40mm, and is taken out from glove box by tantalum pipe, is encapsulated under vacuum conditions in quartz ampoule by tantalum pipe.Subsequently sample is put into diffusion furnace through oversintering and annealing in process, then sample quenched and take out, putting into glove box.Then tantalum pipe is cut, and sample is taken out from tantalum pipe, from sample, cut the sample of one piece of heavily about 50mg, polish flat as thermoanalytical sample;
(3) adopt mould, suppressing external diameter 6mm with the tantalum paper tinsel that thickness is 0.3mm, wall thickness 0.3mm, is highly the tantalum lid of 3mm, and adopt wire cutting machine, by external diameter 6.8mm, the tantalum pipe of wall thickness 0.4mm is cut into the little tantalum pipe that length is 15mm;
(4) sample of well cutting is put into the tantalum pipe of long 15mm one end sealing, and other one end is sealed.The tantalum pipe being sealed with sample is enclosed in vitreosil pipe outward at glove box, then quartz ampoule is put into heat-treatment furnace and anneal, after completing, tantalum pipe is taken out, insert differential scanning calorimetric analysis instrument support and carry out differential thermal analysis (DTA).
Embodiment 3:
For sample preparation and the thermal analyses of Ca-Mg-Mn system, specific implementation process is as follows:
(1) in glove box, adopt magnesium powder (99.5 wt.%), manganese powder (99.5 wt.%), calcium particle (99.5 wt.%), taking volume with electronic balance is 0.3cm
33 samples, after mixing, adopting small-sized electric sheeter to be pressed into diameter 5mm, is highly the cylinder of 6mm;
(2) with argon-arc welder, small column being encapsulated into external diameter is 7mm, wall thickness 0.3mm, and length is in the tantalum pipe of 40mm; Tantalum pipe is taken out from glove box, and is encapsulated under vacuum conditions in quartz ampoule.Subsequently sample is put into diffusion furnace through oversintering and annealing in process, then sample quenched and take out, putting into glove box; Then tantalum pipe is cut, and sample is taken out from tantalum pipe, from sample, cut the fritter of a fritter heavily about 30mg, polish flat as thermoanalytical sample;
(3) adopt mould, suppressing external diameter 6mm with the tantalum paper tinsel that thickness is 0.3mm, wall thickness 0.3mm, is highly the tantalum lid of 3mm, and adopt wire cutting machine, by external diameter 6.8mm, the tantalum pipe of wall thickness 0.4mm is cut into the little tantalum pipe that length is 15mm;
(4) sample of well cutting is put into the tantalum pipe of long 15mm one end sealing, and other one end is sealed, the tantalum crucible being sealed with sample is taken out, bottom is polished flat;
(5) tantalum crucible of good seal is inserted differential scanning calorimetric analysis instrument support and carry out thermal analyses.
Claims (6)
1., containing an alloy sample preparation method for high volatile volatile, high reaction activity element, it is characterized in that, comprise the following steps:
(1) in glove box, take the alloy powder containing high volatile volatile, high reaction activity element, to mix and compressing;
(2) shaping specimen enclosure is entered in tantalum pipe, then tantalum pipe is taken out from glove box, enclose in vitreosil pipe, put into heat-treatment furnace subsequently and carry out sintering and annealing in process;
(3) quartz ampoule taken out rapid quench from heat-treatment furnace and tantalum pipe is taken out, then in glove box, sample being taken out from tantalum pipe.
2. the alloy sample preparation method containing high volatile volatile, high reaction activity element according to claim 1, it is characterized in that, described alloy powder is magnesium alloy powder or Al alloy powder or Zinc alloy powder or manganese alloy powder or strontium alloy powder or yittrium alloy powder or neodymium alloy powder, and wherein the content of high volatile volatile, high reaction activity element magnesium, aluminium, zinc, manganese, strontium, yttrium, neodymium is respectively 99.0wt% ~ 99.99wt%.
3. the alloy sample preparation method containing high volatile volatile, high reaction activity element according to claim 1, is characterized in that, in alloy sample preparation process, keeps sample water oxygen content to be 0.4 ~ 1.0ppm.
4., containing an alloy sample heat analysis method for high volatile volatile, high reaction activity element, it is characterized in that, comprise the following steps:
(1) in glove box, take the alloy powder containing high volatile volatile, high reaction activity element, to mix and compressing;
(2) shaping specimen enclosure is entered in tantalum pipe, then tantalum pipe is taken out from glove box, enclose in vitreosil pipe, put into heat-treatment furnace subsequently and carry out sintering and annealing in process;
(3) quartz ampoule taken out rapid quench from heat-treatment furnace and tantalum pipe is taken out, then in glove box, sample being taken out from tantalum pipe;
(4) sample of sample as differential scanning calorimetric analysis of one piece of heavy 25 ~ 60mg is cut, tantalum lid is suppressed with tantalum piece, by one end of intubating length about 10 ~ 20mm tantalum pipe bottom tantalum lid, and keep the bottom margin of the top of tantalum lid and tantalum pipe to flush, then by tantalum lid and tantalum pipe welded seal in glove box;
(5) in glove box, the sample of well cutting put into tantalum pipe and sealed, the tantalum pipe being sealed with sample is enclosed in vitreosil pipe outward at glove box, then quartz ampoule is put into heat-treatment furnace to anneal, after completing, tantalum pipe is taken out, insert differential scanning calorimetric analysis instrument support and carry out differential thermal analysis (DTA).
5. the alloy sample heat analysis method containing high volatile volatile, high reaction activity element according to claim 4, it is characterized in that, described alloy powder is magnesium alloy powder or Al alloy powder or Zinc alloy powder or manganese alloy powder or strontium alloy powder or yittrium alloy powder or neodymium alloy powder, and wherein the content of high volatile volatile, high reaction activity element magnesium, aluminium, zinc, manganese, strontium, yttrium, neodymium is respectively 99.0wt% ~ 99.99wt%.
6. the alloy sample heat analysis method containing high volatile volatile, high reaction activity element according to claim 4, is characterized in that, in the thermal analyses process of alloy sample, keeps sample water oxygen content to be 0.4 ~ 1.0ppm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105092631A (en) * | 2015-08-07 | 2015-11-25 | 欧优科学仪器南京有限公司 | Thermal analysis method for testing high-activity element alloy material through seal crucible |
| RU2628036C1 (en) * | 2016-06-29 | 2017-08-14 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method of exploring binary barium-lithium alloy and device for its implementation |
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| JPH07181154A (en) * | 1992-03-02 | 1995-07-21 | Ta Instr Inc | Method and equipment of modulation differentiation analysis |
| US5788373A (en) * | 1995-05-19 | 1998-08-04 | Mettler-Toledo Gmbh | Method and apparatus for performing single differential thermal analysis |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105092631A (en) * | 2015-08-07 | 2015-11-25 | 欧优科学仪器南京有限公司 | Thermal analysis method for testing high-activity element alloy material through seal crucible |
| CN105092631B (en) * | 2015-08-07 | 2017-12-01 | 欧优科学仪器南京有限公司 | Utilize the heat analysis method of sealed crucible test high activity element alloy material |
| RU2628036C1 (en) * | 2016-06-29 | 2017-08-14 | Федеральное государственное автономное образовательное учреждение высшего профессионального образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method of exploring binary barium-lithium alloy and device for its implementation |
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Application publication date: 20150610 |